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It is generally accepted that inducing molecular alignment in a polymer precursor via mechanical stresses influences its graphitization during pyrolysis. However, our understanding of how variations of the imposed mechanics can influence pyrolytic carbon microstructure and functionality is inadequate. Developing such insight is consequential for different aspects of carbon MEMS manufacturing and applicability, as pyrolytic carbons are the main building blocks of MEMS devices. Herein, we study the outcomes of contrasting routes of stress-induced graphitization by providing a comparative analysis of the effects of compressive stress versus standard tensile treatment of PAN-based carbon precursors. The results of different materials characterizations (including scanning electron microscopy, Raman and X-ray photoelectron spectroscopies, as well as high-resolution transmission electron microscopy) reveal that while subjecting precursor molecules to both types of mechanical stresses will induce graphitization in the resulting pyrolytic carbon, this effect is more pronounced in the case of compressive stress. We also evaluated the mechanical behavior of three carbon types, namely compression-induced (CIPC), tension-induced (TIPC), and untreated pyrolytic carbon (PC) by Dynamic Mechanical Analysis (DMA) of carbon samples in their as-synthesized mat format. Using DMA, the elastic modulus, ultimate tensile strength, and ductility of CIPC and TIPC films are determined and compared with untreated pyrolytic carbon. Both stress-induced carbons exhibit enhanced stiffness and strength properties over untreated carbons. The compression-induced films reveal remarkably larger mechanical enhancement with the elastic modulus 26 times higher and tensile strength 2.85 times higher for CIPC compared to untreated pyrolytic carbon. However, these improvements come at the expense of lowered ductility for compression-treated carbon, while tension-treated carbon does not show any loss of ductility. The results provided by this report point to the ways that the carbon MEMS industry can improve and revise the current standard strategies for manufacturing and implementing carbon-based micro-devices.

Carbon's electrochemistry depends on its type and microstructure, and how these affect the electrode's electronic density of states. We demonstrate how pyrolysis of electro-mechanically stressed Polyacrylonitrile (PAN) nanofibers, infused with carbon nanotubes, will result in a unique graphitic electrode, which possesses enhanced and multifaceted electrochemical behavior. As corroborated by materials characterization, the microstructure of the stress-activated pyrolytic carbon (SAPC) characteristically contains a high proportion of disorders in the forms of edge planes and embedded heterogeneous nitrogen atoms. These disorders introduce a range of energy states near the Fermi level, yielding enhanced kinetics in the as-synthesized SAPC electrodes. A comprehensive electrochemical study of the SAPC electrode in surface sensitive ([Fe(CN)6]3-/4-), surface insensitive ([IrCl6]2-/3-), and adsorption sensitive (dopamine) redox probes demonstrates 5–14-fold increases in its heterogeneous electron transfer rate compared to regular PAN-based carbon electrodes. The fast kinetics of SAPC electrodes in adsorption sensitive analytes translates into its capability for simultaneous detection of dopamine, uric acid, and ascorbic acid. The results point to a new class of pyrolytic carbon electrodes with an attractive electrocatalytic capacity, geared toward electrochemical sensing platforms.

In this work, we report on a rapid, efficient electrochemical iodine sensor based on mechanically treated carbon nanofiber (MCNF) electrodes. The electrode’s highly graphitic content, unique microstructure, and the presence of nitrogen heteroatoms in its atomic lattice contribute to increased heterogeneous electron transfer and improved kinetics compared to conventional pyrolytic carbons. The electrode demonstrates selectivity for iodide ions in the presence of both interfering agents and high salt concentrations. The sensor exhibits clinically relevant limits of detection of 0.59 µM and 1.41 µM, in 1X PBS and synthetic urine, respectively, and a wide dynamic range between 5 µM and 700 µM. These results illustrate the advantages of the material’s unique electrochemical properties for iodide sensing, in addition to its simple, inexpensive fabrication. The reported iodine sensor eliminates the need for specimen processing, revealing its aptitude for applications in point-of-care diagnostics.

Graphitic carbons' unique attributes have attracted worldwide interest towards their development and application. Carbon pyrolysis is a widespread method for synthesizing carbon materials. However, our understanding of the factors that cause differences in graphitization of various pyrolyzed carbon precursors is inadequate. We demonstrate how electro-mechanical aspects of the synthesis process influence molecular alignment in a polymer precursor to enhance its graphitization. Electrohydrodynamic forces are applied via electrospinning to unwind and orient the molecular chains of a non-graphitizing carbon precursor, polyacrylonitrile. Subsequently, exerting mechanical stresses further enhances the molecular alignment of the polymer chains during the formative crosslinking phase. The stabilized polymer precursor is then pyrolyzed at 1000 °C and characterized to evaluate its graphitization. The final carbon exhibits a uniformly graphitized structure, abundant in edge planes, which translates into its electrochemical kinetics. The results highlight the significance of physical synthesis conditions in defining the structure and properties of pyrolytic carbons.

Catalytic substrate, which is devoid of expensive noble metals and enzymes for hydrogen peroxide (H₂O₂), reduction reactions can be obtained via nitrogen doping of graphite. Here, we report a facile fabrication method for obtaining such nitrogen doped graphitized carbon using polyacrylonitrile (PAN) mats and its use in H₂O₂ sensing. A high degree of graphitization was obtained with a mechanical treatment of the PAN fibers embedded with carbon nanotubes (CNT) prior to the pyrolysis step. The electrochemical testing showed a limit of detection (LOD) 0.609 µM and sensitivity of 2.54 µA cm-2 mM-1. The promising sensing performance of the developed carbon electrodes can be attributed to the presence of high content of pyridinic and graphitic nitrogens in the pyrolytic carbons, as confirmed by X-ray photoelectron spectroscopy. The reported results suggest that, despite their simple fabrication, the hydrogen peroxide sensors developed from pyrolytic carbon nanofibers are comparable with their sophisticated nitrogen-doped graphene counterparts.

In this paper the morphological, mechanical and electrical characteristics of fibers electrospun from a of poly-ε-caprolactone polymer solution with different percentages of graphene nanoplatelets mixed in are reported. The morphology of the fibers was studied under optical and scanning electron microscopes to investigate the interaction of the two phases within the fibers. The scaffolds were characterized to identify the effects of the graphene on the intrinsic properties of the material. The preparation of an optimized suspension of the graphene in the solution was found to be a fundamental factor for enhancing the applicability of the resulting fibers.